CN110867567B - High-safety SiO (silicon dioxide) synthesized by using biomass silicon x Preparation method and application of @ C material - Google Patents
High-safety SiO (silicon dioxide) synthesized by using biomass silicon x Preparation method and application of @ C material Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 25
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 239000010703 silicon Substances 0.000 title claims abstract description 23
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 22
- 239000002028 Biomass Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims description 14
- 239000000377 silicon dioxide Substances 0.000 title claims description 7
- 235000012239 silicon dioxide Nutrition 0.000 title claims description 7
- 238000000034 method Methods 0.000 claims abstract description 18
- 235000007164 Oryza sativa Nutrition 0.000 claims abstract description 12
- 235000009566 rice Nutrition 0.000 claims abstract description 12
- 239000002253 acid Substances 0.000 claims abstract description 10
- 229910052751 metal Inorganic materials 0.000 claims abstract description 9
- 239000002184 metal Substances 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 150000003839 salts Chemical class 0.000 claims abstract description 9
- 238000000498 ball milling Methods 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 7
- 238000004140 cleaning Methods 0.000 claims abstract description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 235000002639 sodium chloride Nutrition 0.000 claims description 12
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 6
- 238000005554 pickling Methods 0.000 claims description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 5
- 230000001681 protective effect Effects 0.000 claims description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 239000001103 potassium chloride Substances 0.000 claims description 4
- 235000011164 potassium chloride Nutrition 0.000 claims description 4
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims description 2
- 235000017491 Bambusa tulda Nutrition 0.000 claims description 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 2
- 235000013162 Cocos nucifera Nutrition 0.000 claims description 2
- 244000060011 Cocos nucifera Species 0.000 claims description 2
- 244000082204 Phyllostachys viridis Species 0.000 claims description 2
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 239000011425 bamboo Substances 0.000 claims description 2
- 239000001110 calcium chloride Substances 0.000 claims description 2
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 2
- 229910052736 halogen Inorganic materials 0.000 claims description 2
- -1 halogen salt Chemical class 0.000 claims description 2
- 239000010903 husk Substances 0.000 claims description 2
- 239000011780 sodium chloride Substances 0.000 claims description 2
- 239000010902 straw Substances 0.000 claims description 2
- 240000007594 Oryza sativa Species 0.000 claims 1
- 239000000047 product Substances 0.000 abstract description 13
- 241000209094 Oryza Species 0.000 abstract description 11
- 238000005406 washing Methods 0.000 abstract description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 5
- 239000000203 mixture Substances 0.000 abstract description 5
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 abstract description 4
- 239000006227 byproduct Substances 0.000 abstract description 4
- 229910052799 carbon Inorganic materials 0.000 abstract description 4
- 229910052744 lithium Inorganic materials 0.000 abstract description 4
- 239000011248 coating agent Substances 0.000 abstract description 2
- 238000000576 coating method Methods 0.000 abstract description 2
- 239000011261 inert gas Substances 0.000 abstract description 2
- 239000010406 cathode material Substances 0.000 abstract 1
- 239000002245 particle Substances 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 44
- 238000005245 sintering Methods 0.000 description 6
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 5
- 229910001416 lithium ion Inorganic materials 0.000 description 5
- 239000007773 negative electrode material Substances 0.000 description 4
- 238000006722 reduction reaction Methods 0.000 description 4
- 239000002210 silicon-based material Substances 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000010000 carbonizing Methods 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000009831 deintercalation Methods 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- 208000019901 Anxiety disease Diseases 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000036506 anxiety Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000011148 calcium chloride Nutrition 0.000 description 1
- 239000000599 controlled substance Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
Images
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention provides high-safety SiO synthesized by biomass silicon x A preparation method of a @ C material comprises the following steps: acid washing rice hull ash, taking a proper amount of the rice hull ash to carbonize in an inert atmosphere, mixing and ball-milling the carbonized product, metal powder and molten salt uniformly, placing the mixture in a furnace, introducing inert gas, reacting at a high temperature, acid washing and cleaning a byproduct to obtain a product which is SiO x @ C material. The method has the advantages of simple and easy process, rich and cheap raw materials, higher safety than magnesiothermic reduction, and capability of obtaining SiO x The @ C particles have a porous structure, are uniform in carbon coating and good in rate capability, and can be applied to the field of lithium battery cathode materials.
Description
Technical Field
The invention belongs to the technical field of new energy material preparation, and particularly relates to high-safety SiO (silicon dioxide) synthesized by biomass silicon x A preparation method of the @ C material.
Background
The method improves the specific energy of the power battery, and is the most effective way for solving the mileage anxiety of the electric automobile at the present stage. Authoritative data show that the lithium ion power battery is required to reach the development target of 300 W.h/kg in 2020, and the only feasible technical route is as follows: the high-nickel ternary positive electrode material NCM 811, NCA or lithium-rich manganese base is matched with the silicon-based negative electrode material.
Research shows that the specific energy of the lithium ion battery can be improved by 15% when the specific capacity of the negative electrode material is increased by 500 mA.h/g. The theoretical specific capacity of the silicon-based negative electrode material can reach 4200 mA.h/g to the maximum extent, is 10 times of the capacity of the traditional graphite negative electrode, has the advantages of rich reserves, low cost, environmental friendliness and the like, and is the first choice of the negative electrode material of the high-specific-energy lithium ion battery. Silicon-based materials that can be used as the negative electrode include: elemental silicon (Si) and silicon monoxide (SiO) x ) Silicon dioxide (SiO) 2 ) Silicon carbide (SiC), etc., wherein the introduction of oxygen can significantly improve the stability of the silicon-based material during the lithium ion deintercalation process.
Conventional SiO x The material of @ C is prepared by mixing simple substance silicon and silicon dioxide at high temperature above 1300 deg.C, neutralizing under vacuum condition, and rapidly cooling and crystallizing to obtain SiO x Then SiO x And (5) carrying out carbon coating. Such as CN 2The 01810059105.2 patent states that the method has harsh synthesis conditions and high requirements on equipment, and is difficult to realize large-scale industrial production. In addition, the method for obtaining the elemental silicon by biomass magnesiothermic reduction is also widely applied, for example, as described in patent CN 201811476229.7, but since magnesium powder is a flammable and explosive controlled drug, only a small amount of experiments can be performed, and large-scale production is not suitable. The invention mainly aims to adopt safer aluminum powder, copper powder, iron powder and the like to carry out metallothermic reduction reaction, change the molar ratio of biomass silicon to metal and change the synthesis conditions to change SiO x The value of x in @ C (0 < x < 2) gives SiO having more excellent properties x @ C material. The whole preparation process is carried out in an inert atmosphere, so that the biomass carbon is kept, the biomass body structure is maintained, and the conductivity, the cycle performance and the rate performance of the material are improved from the inside of the material structure.
Disclosure of Invention
The invention aims to provide a high-safety SiO synthesized by biomass silicon x Method for preparing @ C material for improving SiO x Rate capability and circulation stability of @ C material. The biomass carbon is reserved to achieve the purpose of improving SiO x The purpose of the conductivity and cycling stability of the @ C material.
In order to achieve the above purpose, the solution of the invention is:
1) Mixing a biomass silicon source, pickling and drying, placing in a furnace, introducing protective gas, and reacting for a certain time at a certain temperature to obtain a product A;
2) Mixing the product A and metal powder according to a certain proportion, adding a certain amount of fused salt, ball-milling uniformly, placing in a furnace, introducing protective gas, reacting for a certain time at a certain temperature, pickling and drying to obtain a product B, wherein the product B is SiO x @ C material.
The biomass silicon source is one or more than two of coconut shells, rice husks, bamboo leaves and straws.
The acid used for acid cleaning is one or more than two of hydrofluoric acid, hydrochloric acid, phosphoric acid and sulfuric acid, and the concentration is 0.1-10 mol/L.
In the sintering process in the step 1), the sintering temperature is 400-700 ℃, and the sintering time is 2-12 hours.
The metal powder is one or more than two of aluminum powder, copper powder, magnesium powder and iron powder, and the molar ratio of silicon to the metal powder in the biomass silicon source is 0.5-1.
The molten salt is halogen salt and comprises one or more than two of sodium chloride, potassium chloride, zinc chloride, calcium chloride and sodium bromide, and the mass ratio of the molten salt to the biomass silicon source is 0.5-5.
The rotating speed of the ball milling process in the step 2) is 100-800 r/min, and the time is 0.5-8 hours.
In the sintering process, one or more than two of inert gases of nitrogen, argon and hydrogen-argon mixed gas are adopted.
In the step 2), the sintering temperature is 600-1000 ℃, and the sintering time is 2-12 hours.
The invention has the advantages that: aiming at the danger of the magnesiothermic reduction method, the invention adopts safer aluminum powder, copper powder, iron powder and the like to carry out metallothermic reduction reaction, so that the reaction can be produced in a larger scale. Because the introduction of oxygen can obviously improve the stability of the silicon-based material in the lithium ion deintercalation process, the invention synthesizes SiO by changing the molar ratio of biomass to metal x And the stability of the silicon-based material in the charging and discharging process of the battery is enhanced due to the non-simple substance silicon. According to the invention, molten salt melting is adopted to absorb heat to control the reaction temperature, so that the structure that the original biomass silicon is naturally embedded in organic matters is reserved, and the stability and rate capability of the material are enhanced.
SiO Using the invention x The @ C material has excellent stability, can improve the conductivity of the silicon dioxide material, improves the rate capability, and is beneficial to the industrialization process of the power battery. The controllable SiO of the invention x The oxygen content of the material @ C, and the method is simple and controllable, and is suitable for industrial production.
Drawings
FIG. 1 shows SiO with and without molten salt, which is provided in comparative example 1, which is example 1 of the present invention x The X-ray diffraction contrast spectra of the @ C-800 material.
FIG. 2 shows a synthetic SiO solid provided in example 1 of the present invention x Lithium battery cycle performance diagram of @ C-800 material。
Detailed Description
Example 1
Pickling rice hull ash, carbonizing 5g at 600 ℃ for 1 h under nitrogen, mixing the carbonized product with 0.2g of aluminum powder and 3g of potassium chloride, ball-milling uniformly, placing in a furnace, introducing nitrogen, keeping the temperature at 800 ℃ for 5 h, pickling and cleaning by-product Al 2 O 3 To obtain the product of SiO x The material @ C; the XRD of the product is shown in figure 1, and the electrochemical performance of the lithium battery is shown in figure 2.
Example 2
Acid washing rice hull ash, taking 5g of rice hull ash, carbonizing the rice hull ash for 1 hour under nitrogen, mixing the carbonized product with 0.3g of copper powder and 3g of potassium chloride, ball-milling the mixture evenly, putting the mixture into a furnace, introducing nitrogen, keeping the temperature at 900 ℃ for 4 hours, and acid washing to clean a by-product CuO to obtain a product SiO x @ C material.
Comparative example
Acid washing rice hull ash, taking 5g of the rice hull ash, carbonizing the rice hull ash for 2 hours at 500 ℃ under nitrogen, mixing the carbonized rice hull ash and 0.2g of aluminum powder, ball milling the mixture evenly, putting the mixture into a furnace, introducing nitrogen, keeping the temperature for 5 hours at 800 ℃, and acid washing and cleaning a byproduct Al 2 O 3 To obtain the product of SiO x The material @ C; the product XRD is shown in figure 1.
Claims (5)
1. SiO (silicon dioxide) x The preparation method of the @ C material is characterized by comprising the following steps: the method comprises the following steps:
1) Mixing a biomass silicon source, pickling and drying, placing in a furnace, introducing protective gas, and reacting for a certain time at a certain temperature to obtain a product A;
2) Mixing the product A and metal powder according to a certain proportion, adding a certain amount of molten salt, uniformly ball-milling, placing in a furnace, introducing protective gas, reacting for a certain time at a certain temperature, pickling and drying to obtain a product B, wherein the product B is SiO x The material @ C;
the molten salt is halogen salt and comprises one or more than two of sodium chloride, potassium chloride, calcium chloride and sodium bromide, and the mass ratio of the molten salt to the biomass silicon source is 0.5-5;
in the step 2), in the process of reacting at a certain temperature for a certain time, the certain temperature is 600-1000 ℃, and the certain time is 2-12 hours;
the biomass silicon source is one or more than two of coconut shells, rice husks, bamboo leaves and straws;
the metal powder is one or more than two of aluminum powder, copper powder and iron powder;
the molar ratio of silicon to metal powder in the biomass silicon source is 0.5-1.
2. SiO as claimed in claim 1 x The preparation method of the @ C material is characterized by comprising the following steps: the acid used for acid cleaning is one or more than two of hydrofluoric acid, hydrochloric acid, phosphoric acid and sulfuric acid, and the concentration is 0.1-10 mol/L.
3. SiO as in claim 1 x The preparation method of the @ C material is characterized by comprising the following steps: in the step 1), the reaction is carried out at a certain temperature for a certain time, wherein the certain temperature is 400-700 ℃, and the certain time is 2-12 hours.
4. SiO as in claim 1 x A preparation method of the @ C material is characterized by comprising the following steps: the rotation speed of the ball milling process in the step 2) is 100-800 r/min, and the time is 0.5-8 hours.
5. SiO as claimed in claim 1 x The preparation method of the @ C material is characterized by comprising the following steps: the protective gas in the step 1) or the step 2) is one or more than two of nitrogen, argon and hydrogen-argon mixed gas.
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| CN112259737B (en) * | 2020-10-27 | 2021-05-07 | 成都新柯力化工科技有限公司 | Preparation method of mesoporous spherical silicon oxide negative electrode material of lithium battery |
| CN112397701A (en) * | 2020-11-20 | 2021-02-23 | 江苏科技大学 | Rice husk-based silicon oxide/carbon composite negative electrode material and preparation method and application thereof |
| CN112467125A (en) * | 2020-12-29 | 2021-03-09 | 山东硅纳新材料科技有限公司 | Method for preparing novel silicon-carbon negative electrode material by using rice hull ash |
| CN113178564B (en) * | 2021-04-25 | 2023-01-03 | 陈庆 | Silicon dioxide-carbon composite material and preparation method and application thereof |
| CN114566639A (en) * | 2022-01-17 | 2022-05-31 | 苏州科技大学 | SiO (silicon dioxide)x/C composite material and preparation method and application thereof |
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| CN105932240A (en) * | 2016-05-11 | 2016-09-07 | 武汉科技大学 | Nano-silicon-carbon compound and preparation method and application thereof |
| CN105870422A (en) * | 2016-06-01 | 2016-08-17 | 大连海事大学 | C@SiOx material, preparation method thereof and application of C@SiOx material taken as negative electrode material of lithium ion battery |
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